TWI356048B - - Google Patents
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- TWI356048B TWI356048B TW096145761A TW96145761A TWI356048B TW I356048 B TWI356048 B TW I356048B TW 096145761 A TW096145761 A TW 096145761A TW 96145761 A TW96145761 A TW 96145761A TW I356048 B TWI356048 B TW I356048B
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- Taiwan
- Prior art keywords
- ceramic
- main component
- dielectric
- sample
- temperature
- Prior art date
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- 239000000919 ceramic Substances 0.000 claims description 73
- 239000003985 ceramic capacitor Substances 0.000 claims description 29
- 229910052749 magnesium Inorganic materials 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 3
- 229910052720 vanadium Inorganic materials 0.000 claims description 3
- 229910052684 Cerium Inorganic materials 0.000 claims description 2
- 229910052693 Europium Inorganic materials 0.000 claims description 2
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 2
- 229910052765 Lutetium Inorganic materials 0.000 claims description 2
- 229910052779 Neodymium Inorganic materials 0.000 claims description 2
- 229910052772 Samarium Inorganic materials 0.000 claims description 2
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 2
- 229910052692 Dysprosium Inorganic materials 0.000 claims 1
- 229910052691 Erbium Inorganic materials 0.000 claims 1
- 229910052689 Holmium Inorganic materials 0.000 claims 1
- 229910052771 Terbium Inorganic materials 0.000 claims 1
- 229910052775 Thulium Inorganic materials 0.000 claims 1
- 229910052746 lanthanum Inorganic materials 0.000 claims 1
- 239000000126 substance Substances 0.000 claims 1
- 239000000523 sample Substances 0.000 description 49
- 239000000843 powder Substances 0.000 description 25
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 16
- 239000000203 mixture Substances 0.000 description 16
- 239000001301 oxygen Substances 0.000 description 16
- 229910052760 oxygen Inorganic materials 0.000 description 16
- 239000002994 raw material Substances 0.000 description 16
- 239000012298 atmosphere Substances 0.000 description 15
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 14
- 229910052761 rare earth metal Inorganic materials 0.000 description 11
- 239000003990 capacitor Substances 0.000 description 9
- 239000007789 gas Substances 0.000 description 9
- 150000002500 ions Chemical class 0.000 description 9
- 238000010304 firing Methods 0.000 description 8
- 238000009413 insulation Methods 0.000 description 8
- 238000000034 method Methods 0.000 description 8
- 229910002113 barium titanate Inorganic materials 0.000 description 6
- 239000011812 mixed powder Substances 0.000 description 6
- 229910052788 barium Inorganic materials 0.000 description 5
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 5
- 239000011230 binding agent Substances 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 5
- 238000001354 calcination Methods 0.000 description 5
- 239000004020 conductor Substances 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 239000003989 dielectric material Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- 229910052718 tin Inorganic materials 0.000 description 5
- 229910052797 bismuth Inorganic materials 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000012299 nitrogen atmosphere Substances 0.000 description 4
- 239000007858 starting material Substances 0.000 description 4
- 238000006467 substitution reaction Methods 0.000 description 4
- 229910052726 zirconium Inorganic materials 0.000 description 4
- XOLBLPGZBRYERU-UHFFFAOYSA-N SnO2 Inorganic materials O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 150000001768 cations Chemical class 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(III) oxide Inorganic materials O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 3
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000007747 plating Methods 0.000 description 3
- 239000006104 solid solution Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 2
- 238000004998 X ray absorption near edge structure spectroscopy Methods 0.000 description 2
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Inorganic materials [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 2
- -1 caC03 Inorganic materials 0.000 description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 230000020169 heat generation Effects 0.000 description 2
- 238000010030 laminating Methods 0.000 description 2
- 229910052745 lead Inorganic materials 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052707 ruthenium Inorganic materials 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 208000016952 Ear injury Diseases 0.000 description 1
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- 229910052777 Praseodymium Inorganic materials 0.000 description 1
- 206010036790 Productive cough Diseases 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 238000002056 X-ray absorption spectroscopy Methods 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- YDGGDGXBBJSVKU-UHFFFAOYSA-N butanal ethene Chemical compound C(CCC)=O.C=C YDGGDGXBBJSVKU-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 238000000113 differential scanning calorimetry Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000007606 doctor blade method Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 231100000989 no adverse effect Toxicity 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 210000003802 sputum Anatomy 0.000 description 1
- 208000024794 sputum Diseases 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
- H01G4/06—Solid dielectrics
- H01G4/08—Inorganic dielectrics
- H01G4/12—Ceramic dielectrics
- H01G4/1209—Ceramic dielectrics characterised by the ceramic dielectric material
- H01G4/1218—Ceramic dielectrics characterised by the ceramic dielectric material based on titanium oxides or titanates
- H01G4/1227—Ceramic dielectrics characterised by the ceramic dielectric material based on titanium oxides or titanates based on alkaline earth titanates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/003—Titanates
- C01G23/006—Alkaline earth titanates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
- C01G25/006—Compounds containing, besides zirconium, two or more other elements, with the exception of oxygen or hydrogen
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
- C04B35/49—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/02—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances
- H01B3/12—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances ceramics
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/30—Stacked capacitors
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/50—Solid solutions
- C01P2002/52—Solid solutions containing elements as dopants
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3208—Calcium oxide or oxide-forming salts thereof, e.g. lime
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3215—Barium oxides or oxide-forming salts thereof
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3225—Yttrium oxide or oxide-forming salts thereof
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3227—Lanthanum oxide or oxide-forming salts thereof
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
- C04B2235/3229—Cerium oxides or oxide-forming salts thereof
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- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3239—Vanadium oxides, vanadates or oxide forming salts thereof, e.g. magnesium vanadate
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3262—Manganese oxides, manganates, rhenium oxides or oxide-forming salts thereof, e.g. MnO
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3279—Nickel oxides, nickalates, or oxide-forming salts thereof
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3284—Zinc oxides, zincates, cadmium oxides, cadmiates, mercury oxides, mercurates or oxide forming salts thereof
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Description
1356048 九、發明說明: 【發明所屬之技術領域】 本發明係關於-種介電質H、及使用其之積層陶竟電 容,更詳細係關於一種居裏溫度高且可在175<t程度之高 溫中穩定使用之介電質陶瓷。 & ^ 【先前技術】 作 而成 為本發明主用途之積層陶竟電容一 般以如下方式製造
首先’準備包含介電質陶竞原料之陶:£生片,其係於其 表面具有期望圖案並給與作為内部電極之導電材料。作為 介電質陶瓷,例如可使用以BaTi〇3系為主成分者。•、’ 然後’積層'熱壓接包含給與上述導電材料之陶竟生片 之複數個陶瓷生片,藉此作成一體化之生積層體。 然後, 體。該陶 部電極。 將該生積層體培燒,藉此得到燒結後之陶咖 究積層體之㈣形成有具上料電材料構成之内 接著’在衫積層體之外表面上,以與内部電極之特定 :電氣連接之方式形成外部電極。外部電極例如藉由將包 含導電性金屬粉末及玻璃粉之導電性糊料給與積層體之外 表面上並培燒而形成。如此—來,完成積層陶曼電容。 作為適合積層陶竞電容之介電質陶£,有鈦酸頷 (BaTl〇3)系。例如專利文獻1揭示了一種介電質陶莞,其以 欽酉夂銷為主成分’作為副成分包括Sn〇2、Bi2〇3、Mg〇、 S1O2、La2〇3、Sm2〇3、則2〇3。 126515.doc 1356048 ,專利文獻i之介電質陶兗之居裏溫度低到答15 所以;丨電¥數隨著溫度升高而急減,有不堪高溫區使 用之問題。特別是最近積層陶瓷電容被應用於汽車用途 所以希望於175〇c程度之高溫中仍可穩定使用。因 此’最好居裏溫度至少為l3(rc以上。 因此,專利文獻2中揭示了一種介電質磁器組成物其 將以組成式:(Ba,Sn)Ti〇3表示之鈣鈦礦型化合物作為主成 分’居裏溫度為13〇。(:以上。 在專利文獻2之介電質磁器組成物中,藉由將“作為2價 正離子位於Ba位置,使磁器之居裏溫度上升至13〇tw 上。 再者,一般Sn之4價正離子為穩定狀態,所以在鈦酸鋇 系中通常位於Ti位置。鈦酸鋇之丁丨由Sn置換,則如非專利 文獻1所揭示’在Sn未置換時為120°C之居裏溫度大降至室 溫以下。專利文獻1所揭示之介電質陶瓷之居裏溫度低之 原因也被認為係由於Sn作為4價正離子位於Ti位置。 [專利文獻1]公報特開平3-040962號公報(全文) [專利文獻2] WO 2005/075377號公報(全文) [非專利文獻1]圖崎清、"陶瓷介電質工程學•第3版,, (281 〜283 頁) 【發明内容】 [發明所欲解決之問題] 在專利文獻2中,使Sn作為2價正離子位於Ba位置以取得 高居裏溫度。然而,在高達175°C之高溫時,靜電電容溫 126515.doc 1356048 度特性難以滿足X9R(在_55〜175t:之範圍中以25。〇為基準 之靜電電容之溫度變化在士15%以内)〇 本發明係鑒於該問題點而完成者,提供一種具有高居裏 溫度、在高&75〇C程度之高溫令仍呈穩定之特性並滿足 咖特性之介電質㈣,及使用其之積層陶究電容。 [解決問題之技術手段] 即,本發明之介電質陶究之特徵在於:將以組成式: (Bai-x_yCaxSny)m(Til.zZrz)〇3表示之触礦型化合物泮中前 述x、y、z、m分別滿足❹列“以別卜仏“㈣、 :〇:Γ:2。、。^〇.°5)作為主成分,對於前述主成分 、耳伤包括0.5〜20莫耳份RE(其中RE係選自γ、La、
Ce、Pr、Nd、Sm、Eu、Gd、几 n T , y Ho ' Er > Tm ' Yb 及Lu中之至少一種)作為副成分。 又,最好本發明之介電質陶瓷 之X滿足。.0如。·20β 成刀中表不Ca含有量 上。發月之介電質陶瓷其居裏溫度最好為130。。以
耳:二最:本發明之介電質陶:光對於前述主成分⑽莫 耳伤包3 0.02H莫耳份選自M 分。 甲之至少1種作為副成 又,最好本發明之介電質陶瓷對於 份包含0.3〜4莫耳份選自M 、, 为100莫耳 分。 選自Ha中之至少!種作為副成 記主成分100莫 再者,最好本發明之介電質陶究對於前 126515.doc 切6048 耳份包括〇·2〜5莫耳份Si作為副成分。 再者’本發明之介電質陶瓷也適合將本發明之 曼用於陶瓷層之積層陶瓷電容。 即,本發明之積層陶瓷電容,其特徵在於:對於勺A 數個積層之陶究層及沿其界面形成之複數個層狀内 之陶瓷積層體’為了電氣連接露出於前記陶瓷積層體之 面之内部電極而形成有複數個外部電極,且前述;: 含本發明之介電質陶瓷。 ^ ^ 再者,最好本發明之積層㈣電容其 為Ni。 电蚀之主成分 [發明之效果] 根據本發明,於以鈦酸頻系為主成分之介電質陶兗中, =其Ba位置之—部分被2價正離置換,所以居裏溫 度提高到⑽以上。值得注目的是,因為本發明之介電 質陶瓷作為副成分還包括稀土族元她,所以介電常數 =於溫度之變化可平滑到⑽之高I,結果靜電電容溫 度特性可滿足X9R。 又’ Ba位置之-部分再為⑽置換時,即使將培燒氣氛 之還原度抑制為氧分壓10'1〇-12 Mpa程度,㈣乃充分作 為2價正離子位於Ba位置。&,由於培燒條件之自由度增 加,藉由焙燒條件之調整容易使介電特性改變。 再者,作為副成分,又包括Mn及v中至少丨種,啦、犯 中至/1種4Si時,將本發明之介電質陶究應用於 以犯為主成分之積層㈣電容時,可確保良好之絕緣電陣 126515.doc 1356048 或信賴性。 由以上,藉由使用本發明之介電質陶瓷,可取得適合汽 車用途等在咼溫中使用之積層陶竞電容。 【實施方式】 首先,對本發明之介電質陶瓷主要用途之積層陶瓷電容 進行說明。圖1係表示一般積層陶瓷電容丨之剖面圖。 積層陶瓷電容1具有長方體狀之陶瓷積層體2。陶瓷積層 體2具有複數個積層之介電質陶瓷層3、沿著複數個介電質 陶究3間之界面而形成之複數個内部電極4及5。内部電極4 及5係以延伸到陶:是積層體2之外表面之方式形成,拉出至 陶瓷積層體2之一方端面6之内部電極4與拉出至另一方端 面7之内部電極5在陶:是積層體2之内部,交互配置成經由 介電質陶瓷層3可取得靜電電容。 内部電極4及5之導電材料之主成分可使用鎳、銅、銀 等’從降低成本這點看,以Ni為佳。 為取出前述之靜電電容,在陶瓷積層體2之外表面上且 端面6及7上分別形成有外部電極8及9,以與内部電極4及5 之任一特定者電氣連接。作為外部電極8及9中所含之導電 材料,可以使用與内部電極4及5之情況相同之導電材料, 並且也可使用銀' &、銀-銘合金等。外部電極8及9係藉 由、”。與在該種金屬粉末添加玻璃粉而得到之導電性糊料, 並將其焙燒而形成。 又,外部電極8及9上,根據需要,分別形成包含鎮、銅 等之第1電錄層10及11,再在其上分別形成包含焊料錫 126515.doc 1356048 等之第2電鍍層12及13。 其次,對本發明之介電質陶瓷之詳細進行說明。 本發明之介電質陶瓷之組成,其主成分為以組成式: (Bai-x-yCaxSnj^n^Tii-zZrJO3表示之妈鈦礦型化合物,前述 X、y、z、m為 0.990$mg 1.015、osxgo.20、〇 〇2gyg 0.20、0 $ 0.05。 在此,Sn主要作為2價正離子位於Ba位置,而幾乎不位 於Ti位置。鈦酸鋇之居裏溫度約i2〇〇c,Sn對該Ba位置置 換量越增加居裏溫度越上升,置換量y達到〇〇2以上時居 裏溫度達到1 30°C以上。又,ca主要也作為2價之正離子位 於Ba位置。然而,因為Ca之位置對於居裏溫度之增減無大 幫助,所以在不損害本發明目的之範圍内,可以若干量存 在於晶界或位於Ti位置。 此外,Ti之一部分也可由Zr置換。然而,置換量z超過 〇·〇5時,居裏溫度會顯著下降,與本發明之目的相反。最 好z值小,〇·〇1以下則更佳。
Ba位置對於7^位置之莫耳比m若為〇 990M 〇15範圍,則 可保持穩定之燒結性與絕緣性。 且,應注目的是,本發明之介電質陶瓷作為副成分包含 稀土族元素RE。若對於主成分1〇〇莫耳份,使其含有〇 5莫 耳伤以上之RE,則介電常數對於溫度之變化變得平滑,結 果靜電電容溫度特性滿足X9R特性。雖然該理由並非— 疋但推測為晶格容積因Sn固溶於Ba位置而變化,向此處 添加稀土族元素RE,而對於晶格向增強強介電性,即正方 126515.doc 1356048 晶性之方向施加應力。萁 ^ 一刀另一方面,不存有Sn時或Sn位於Ti 4置時〗此看見如上述之效果。此外,含有量之上 限’為高度維持介電常數,以20莫耳份為佳。 又本發明中之ca具有促進Sn向Ba位置固溶之作用。 此時,若料時之氧分以1G.1GMPa^程度,則Sn容易 固冷於Ba位置。能較高地設定培燒時之氧分Μ,與提高材 料設計與元件設計之自由度相關。該些效果於置換量X為 〇·02以上顯現。Χ之上限,為確保Ca之均勻固溶,以0.20莫 耳份為佳。 ' 又,本發明中,居裏點為130°C以上為佳。本發明之介 電質陶瓷中,#由確認居裏溫度為13〇。。,以知曉Sn位於 Ba位置。如前述非專利文獻丨亦所示,〜位於丁丨位置時, 居裏溫度從12〇它開始大降。 又本發明之介電質陶瓷因Ba位置之一部分為Sn所置換 而有利於取得高居裏溫度,但不希望包含很多降低居裏溫 成刀即使添加降低居襄溫度之成分時,也最好藉由 增多對Ba位置之Sn置換量等手段以彌補。 相反地’除Sn以外’作為提升鈦酸鋇之居裏溫度之元 素’可列舉Pb及Bi。然而,因為Pb或Bi之耐還原性非常 弱’故非常難適用於積層陶瓷電容。 由以上’對於本發明之介電質陶瓷,藉由確認居裏溫度 為13〇°C以上,實質上可證明Sn作為2價正離子存在於Ba位 置。 又’也可藉由X射線吸收分光法之一種XANES(x-ray 126515.doc 11 1356048
Absorption Near Edge Structure)來確認 Sn作為 2價正離子存 在於Ba位置。即,在本發明之介電質陶瓷中,指定相當於 Sn之K殼電子之激發能量之X射線吸收端,藉由將表示該又 射線吸收端之能量值與Sn2+、Sn4+等Sn離子之參考值比 較,則可知曉介電質陶瓷中Sn之價數。 又,關於該XANES測定,為提高測定精度與感度,要求 入射X射線之強度高且波長連續性高。如此一來,對於入 射X射線之光源以使用放射光為佳。
又,本發明之介電質陶瓷除稀土族元素RE以外也可加 入各種副成分。近年,在使用以川為主成分之内部電極之 積層陶瓷電容中,因為小型化,陶瓷層之日益薄層化進 展。因此,在藉由還原、氣氛培燒而得到之薄層S之積層陶 瓷電容中,為得到足夠之絕緣電阻或信賴性,最好加入各 種副成分。 n 碲到成分含有Μη及V中至
^ -種時’在使用以Ni為主成分之内部電極之薄層品之 電容中,可取得足夠之絕緣電阻。為在薄層品確保 良好<5賴性,含有量對# ± 、 ’、 〇〇] 里子於主成分_莫耳份,最好為 〇·〇ι〜1莫耳份。 q 自:為其他例子’本發明之介電質陶瓷作為副成分含有選 自Mg、Ni、Zn中至 韦選 部電極之薄層。… 在使用以Ni為主成分之内 阻之積層陶究電容中,可取得足夠之絕緣電 :耳::::確保良好信賴性,含有量對於主成分= 六今伪,最好為0·3〜4莫耳份。 1265I5.doc -12· 1356048 又,本發明之介電質陶兗作為副成分含有si,例如Si〇 時,即使在還原线培燒中,也容易以更低溫燒結。含有2 量對於主成分100莫耳份,〇.2〜5莫耳份為宜。 然後,對本發明之介電質陶瓷之製造方法進行說明。 首先,對介電質陶变用之陶-充原料之製法進行說明。。主 成分Ca,sn)(Ti ’ Zr)03粉末例如可藉由固相法得 到,該固相法係混合氧化物粉末或碳酸化物等初始原料, 並熱處理合成所得之混合粉體。 w
然而,本發明之介電質陶究為了最終Sn作為2價正離子 位於Ba位置,有必要將通常4價且穩定之Sn還原到2價。例 如,在合成(Ba,Ca,Sn)(Ti, Zr)〇3之際之熱處理合成 時’最好將氣氛設為還原氣氛。具體而言,最好將氧分厘 設在10·10 MPa以下。 又,Sn之初始原料為了切實將“固溶於主成分,最好與
Ba或Ti之初始原料共同混合。含有㈣,也同樣最好與Ba 或Ti之初始原料共同混合。 如此知到之(Ba , Ca,Sn)(Ti,Zr)〇3粉末中混合作為稀 土族元素之初始原料之奸2〇3 ,根據需要混合Mn〇、 MgO、Si〇4副成分,可得到陶£原_。該些副成分也並 不特別限疋原料之形態或化合物之種類。 使用由上述方法得到之陶£原料,藉由與習知積層陶瓷 電容之製造方法相同之方法,得到生積層|^在培燒生積 層體時’焙燒時之氣氛有必要設為還原氣氛。為使Sn作為 2價正離子位於Ba位置,該還原氣氛之氧分壓可靠的是 126515.doc -13- 1356048 10" MPa以下,伸c人古θ ί- La 3有置乂為〇 〇2以上時,也可以為 10_1G〜10_12 MPa程度。 又,以位置總量對於Ti位置總量之莫耳比m不必-定在 該些初始原料調合時即滿例如,可以在主成分粉末之 初始原料調合時,先若干少量地調合m,而在(Ba,^ Sn)(Ti ’ Ζι·)〇3合成後,添加不足分之以成分之初始原料。 此場合,作為不足分而添加之仏成分,藉由培燒,主要固 溶於主成分中而滿足期待之m值。 並且,焙燒而得到陶瓷積層體後,藉由與習知同樣之方 法得到積層陶瓷電容。 又積層陶瓷電容之介電常數等介電特性可藉由與習知 同樣之方法冲估。對於居裏溫度,最好提取積層陶瓷電容 之介電常數之溫度變化,以介電常數極大之溫度為居裏 點。即使介電常數對於溫度變化之極大點不明確時,也可 藉由查詢由X射線繞射表示之結晶晶格之c/a軸比之溫度變 化’將正方晶與立方晶之邊界溫度設為居裏溫度。又可 藉由差示掃描熱量測定法檢測由正方晶與立方晶之間相轉 移而產生之發熱峰值,而將該發熱峰值之產生溫度設為居 長溫度。 [實施例] 以下’對本發明之介電質陶瓷、及使用其之積層陶瓷電 容之實施例,以實驗例1〜3進行說明。 [實施例1 ]本實驗例係藉由以Ni為内部電極之積層陶瓷 電容來查驗RJE對於主成分(Ba,Ca,Sn)(Ti,Zr)03之效果。 126515.doc 14 1356048 首先作為初始原料準備有BaC〇3、Ti〇2、caC03、 Sn02。將匕們調合成如組成式:(Ba。“ca。wu】。】叫 表不之,’且成。將該調合粉以球磨機混合粉碎乾燥後得 到混合粉體》 將該混合粉體於台人\了 ^ 、匕3 N2-H2混合氣體之氧分壓10·ι〇 MPa 氣氛中4 1000 c下熱處理合成2小時而得到以 (Bk85Ca^Sn().05)1〇lTi〇3 為主成分之粉末。 」後對乂 (Ba〇.85Ca0_10Sn〇.05)101Ti〇3為主成分之粉末, 以對於(Ba0.85Ca〇 1〇Sn〇 〇5)i 〇iTi〇3i〇〇莫耳份,、
Mg、Si分別為a莫耳份、〇5莫耳份、ι〇莫耳份、2〇莫耳 份之方式’調合Dy2〇3、MnC〇3、MgC〇3、叫,並於溶 财使其混合。此時,改變Dy之含有〔量a,使其變化成表i 之试料編號1〜8之試料之值。',日人你 值 此σ後’幹式粉碎該粉末, 作為陶瓷原料。 將該陶瓷原料以乙醇為溶劑,涞 合w 添加多孔乙烯丁醛系結合 劑’混合粉碎後得到浆料。將节婿姓〜m ^ 將及漿枓利用刮刀法形成片 材’得到厚度7 μιη之陶瓷生片。 絲網印刷以Ni為主成分之導電性糊料於上述陶究生片之 表面,形成用以構成内部電極之導電糊料層…電性糊 料層被拉出側相異之方式積層形成有該導電糊料層之陶究 生片,得到生積層體。 /將該生積層體於氮氣氛中以35(rc加熱,使結合劑燃燒 後,在包含Η2·Ν2_Η2〇氣體之氧分壓1〇.u.5 Mpa之氣氛中, 以表1所示之溫度保持2小時,得到經焙燒之陶瓷積層體。 126515.doc -15· 1356048 在該陶變積層體之兩端面上塗佈含有BU_si_Ba〇系玻 璃粉’並以Cu為主成分之導電性糊料,於氮氣氛中以 6〇旳培燒’而形成與内部電極電氣連接之外部電極。再 者,為使焊接性良好’在外部電極上形成⑽層及鑛Sn 層。 •如此得到之積層陶莞電容i之外形尺寸為長20 mm、寬 • U mm、厚0.5 mm,介於内部電極間之㈣層之厚度為5 μΠ1 ’内部電極之金屬厚度為G.5 μιη,對靜電電容有效之陶 瓷層數為5 ’陶瓷層每層之對向電極面積為ι 3χΐ〇·、2。如 以上’得到試料編號1〜8之評估試料。 ::、後在25 C中施加1分鐘30 kv/mm之直流電壓以測定 試料編號卜8之試料之絕緣電阻,由絕緣電阻值求得電阻 率P °將log(CT/Qm)值表示在表}中。 並且在25C中在1 kHz、〇.2 kVrms之交流電場下評估 介電常數εΓ,將其值表示在幻中。又,在_55〜175^之範 φ 圍下測定靜電電容,將以25°C為基準在175°C之靜電電容 之變化率作為「靜電容量變化率(%)"表示在表1中。此 時也—併表不是否滿足X9R特性(在_55〜175T:之範圍中 以25 c為基準之靜電電容之溫度變化在士15%以内)之判定 / 結果。 又’在-55〜200 C之範圍内測定靜電電容之溫度變化, 將靜電電容保持極大時之溫度定為居裏溫度,表示在表1 中。 此外’測定在溫度175〇c且施加電場2〇 kv/mm之條件下 126515.doc j:>6〇48 之鬲溫負荷壽命,將其平均故障時間(MTTF :單位h)之結 果表示在表1中。此時之故障為電阻值成為1〇6ω以下之 時。 [表1]
試料編號!之試料不含稀土族元素,而試料編號2之試料 之稀土族元素含有量很少,所以靜電電容溫度特性不滿足 X9R特性。 试料編號3〜7之試料藉由Dy之作用,靜電電容滿足x9r 特性,且e r也顯示1 0 〇 〇以上。 試料編號8之試料之巧之含有量過多,所以訂值小於 1000。 [實驗例2]本實施例係在以Ni為内部電極之積層陶竞電 容或單板電容之中,查驗Sn含有量及固溶狀態給與本發明 之主效果之影響。 首先以組成式.(Bai χ yCaxSn^丨。之表示表2之試 料編號11〜24之x、y值之組成之方式調合初始原料 3 2 CaC〇3、Sn〇2。將該調合粉在球磨機中混 合粉碎並乾燥後,得到混合粉體。 126515.doc 1356048 將該混合粉體在大氣中或包含沁_仏混合氣體之表2所示 之氧分壓氣氛中,在1000。(:下熱處理合成2小時,得到以 (BaiiyCaxSiiyh·。丨Ti03為主成分之粉末。 然後,對於以(Bai_x.yCaxSny)丨·。丨Ti〇3為主成分之粉末, 以對於(Ba丨.x.yCaxSny)1()lTi〇3l〇〇莫耳份,巧、Mn、、
Si分別為3莫耳份、〇 5莫耳份、1〇莫耳份、2 〇莫耳份之 方^調合Dy2〇3、MnC〇3、MgC〇3、叫,並使其在溶劑 鲁巾混合。混合後,將該粉末乾式粉碎得到陶竟原料粉末。 利用該陶瓷原料,經過與實驗例丨相同之步驟,得到與 實驗例1相同構成之生積層體。 又,僅試料編號12之試料不製作生積層體,而製成單板 成形體。#,將陶究原料粉末與丙烯系有機結合劑共同濕 式混合,將其後乾燥、造粒之粉體於196 Μρ&之壓力下沖 壓成形,藉此得到12 ππηφ直徑、厚度i麵之圓板成形 體。 • 將該些生積層體及圓板成形體在氮氣氛十以35(TC加熱 並使結合劑燃燒後,在大氣中或包括Η2·Ν2_Η2〇氣體之表2 . 所示之氧分壓還原性氣氛中,以表2所示之培燒溫度保持2 小時,得到經燒結之陶瓷積層體及圓板狀燒結體。 • 對於所得之陶兗積層體,經過與實驗例丨相同之步驟, 得到具有與實驗例丨相同構成之積層陶瓷電容之試料。 對於試料編號之圓板燒結體,在其兩主面上形成八§蒸 鍍膜’將其作為外部電極。如此得到之單板陶究電容之外 形尺寸為10 mm直徑、厚度0.8 mm。 126515.doc 1356048 對於如以上得到之試料編號11〜24之試料,以與實驗例1 相同之方法,評估電阻率σ之log(a/Qm)、ει·、靜電電容之 溫度變化率、高溫負荷試驗之MTTF、居裏溫度,並將其 結果表示在表2中。 [表2]
試料 編號 X y 熱處理合成 時氧分壓 (MPa) 培燒時 氧分壓 (MPa) 焙燒 溫度 (°C) log (σ/Ωιη) £ Γ MTTF (h) 居裏 溫度 (°C) 靜電電容 電變化率 (%) X9R 判定 氺11 0.10 0.00 lxlO·10.0 lxlO·"5 1050 12.1 1300 30 120 -25 X 氺12 0.10 0.02 大氣中 大氣中 1050 11.3 1200 - 105 -50 X 氺13 0.10 0.02 大氣中 大氣中 1050 11.2 1200 20 105 -50 X 14 0.10 0.02 lxlO'100 lxl〇·"5 1050 11.8 1300 30 130 -15 〇 15 0.10 0.07 lxlO-101 lxlO·11.5 1050 11.8 1300 35 145 •12 〇 16 0.10 0.15 lxlO'102 lxlO'115 1050 11.9 1000 35 150 -10 〇 17 0.10 0.20 lxlO·10.3 lxlO-11*5 1050 12.1 1000 35 155 -8 〇 氺18 0.10 0.30 lxlO·10.4 lxlO·11.5 1050 12.1 450 - 165 -3 〇 19 0.00 0.05 lxlO·10.5 lxlO·11.5 1050 12.3 2000 20 130 •15 〇 20 0.02 0.05 1x10.丨06 lxlO'115 1050 12.3 1800 25 130 -15 〇 21 0.05 0.05 lxlO·10.7 lxlO·11.5 1050 12.1 1500 30 135 -15 〇 22 0.10 0.05 lxlO·108 lxlO-".5 1050 12.1 1300 40 140 -14 〇 23 0.20 0.05 lxlO·10.9 lxlO'115 1050 11.8 1000 40 140 •14 〇 氺24 0.22 0.05 lxl〇·'010 lxl〇·'15 1050 11.8 600 - 140 -14 〇 試料編號11之試料不含有Sn,所以儘管對於主成分1 00 莫耳份含有3莫耳份以上稀土族元素Dy,仍不滿足X9R特 性。 試料編號12之試料以Sn為y=0.02之方式調合,儘管對於 主成分100莫耳份含有3莫耳份以上稀土族元素Dy,仍不滿 足X9R特性。此由居裏溫度小於130°C,表明Sn主要位於Ti 位置。被認為是因在主成分粉末之熱處理合成時及焙燒時 •19- 126515.doc 1356048 氧分壓高。 試料編號13之mSn為y=G G2之方式調合 主成分刚莫耳份含有3莫耳份以上稀土族元素以,仍不滿 足X9R特性。此由居裏溫度小於13代,表明〜主要位於们 位置。被認為是因在主成分粉末之熱處理合成時氧分遂 高0 試料編號M〜17之試料滿足X9R特性,取得嶋以上之 "裏溫度達到啊以上,表明〜主要位於仏位置。 但是’如試料18所示Sn含有量y超過⑽,則^下降為小 於 1000 » 忒料編唬19〜23之試料係改變Ca量之試料與試料編號 —樣,滿足X9R特性,取得1〇〇〇以上之^。但是,如 試料24所示Ca含有量y超過0.02,則εΓ下降為小於1000。 因為試料編號19之試料不含Ca,所以需要比其他試料 降低焙燒時之氧分壓,但實用上是沒有問題的程度。 [實驗例3 ]本實驗例係對於同一製造條件下之犯内部電 極之積層陶瓷電容,觀察到副成分之種類及含有量給與諸 特性之影響。 首先,作為初始原料,準備有BaC03、Ti02、CaC03、 Sn02將匕們調合成組成式:(Ba0.85Ca0.〗0Sn0.05)mTiO3之 表3之试料編號3 值表示之組成。將該調合粉以球 磨機咸合粉碎、乾燥後,得到混合粉體。 將該混合粉體在包含N2-H2混合氣體之氧分壓i〇_1Q MPa 之氣现中’在1000<t下熱處理合成2小時,得到以 126515.doc -20- 1356048 (以〇85〇压〇_1。811〇。5)1111^03為主成分之粉末。 然後,對於以(BaowCa^SnowhTih為主成分之粉 末,以稀土族元素RE對於主成分100莫耳份之含有莫耳^ a、選自Μη及V中之至少1種之含有莫耳份5、選自 犯、Zn中之至少⑽之含有莫耳份c、Si之含有莫耳份:分 別為表3之試料編號31〜71所示之值之方式,調合、
La203、C〇2、Pr6〇丨丨、Nd2〇3、Sm2〇3、如办叫〇3、
Tb2〇3、Dy2〇3、H〇2〇3、以2〇3、Tm2〇3、外办、[η办、
MnC〇3、V2〇3、MgC〇3、、Zn〇、,並使其2在3溶 劑中混合°將混合後並乾燥而得到之粉末乾式粉碎,得到 陶瓷原料粉末。 利用該陶瓷原料,經過與實驗例1相同之步驟,得到與 實驗例1相同構造之生積層體。 將5亥生積層體在氮氣氛中以35G°C加熱並使結合劑燃燒 後,在包含H2-N2_H20氣體之氧分壓1〇-n.5 Mpa之還原性氣 "" 、表3所示之培燒溫度保持2小時,得到經培燒之陶 瓷積層體。 於”亥陶瓷積層體經過與實驗例丨相同之製造條件形成外 4電極得到試料編號3 1〜71之積層陶瓷電容之試料。 對於如以上得到之試料編號3 1〜71之試料,以與實驗例1 才Π之方法β平估電阻率σ之l〇g(a/Qm)、ει*、靜電電容之 溫度變化率、古,、田Α # 同,皿負何試驗之MTTF、居裏溫度,並將其 結果表示在表3中。 126515.doc 1356048 [表3]
試料 編號 m a b c d 焙燒 温度 CC) log (σ/Ωπι) ετ MTTF (h) 居裏溫度 ΓΟ 靜電電容 變化率 (%) X9R 判定 氺31 0.980 Dy3.0 Mn 0.50 Mg 1.0 2.0 1050 9.7 1600 - - - - 32 0.990 Dy3.0 Mn 0.50 Mg 1.0 2.0 1050 12.3 1300 40 143 -12 〇 33 1.000 Dy3.0 Mn 0.50 Mg 1.0 2.0 1050 12.1 1300 40 144 -12 〇 34 1.015 Dy3.0 Mn 0.50 Mg 1.0 2.0 1050 12.1 1100 30 140 -15 〇 氺35 1.020 Dy3.0 Mn 0.50 Mg 1.0 2.0 1200 - - - - - - 36 1.010 Dy3.0 Mn 0.01 Mg 1.0 2.0 1050 6.0 - - - - - 37 1.010 Dy3.0 Mn 0.02 Mg 1.0 2.0 1050 11.6 1200 25 145 -12 〇 38 1.010 Dy3.0 MnO.lO Mg 1.0 2.0 1050 11.7 1300 50 145 -12 〇 39 1.010 Dy3.0 Mn 0.60 Mg 1.0 2.0 1050 11.8 1300 50 145 •12 〇 40 1.010 Dy3.0 Mn0.80 Mg 1.0 2.0 1050 11.6 1300 50 145 -12 〇 41 1.010 Dy3.0 Mn 1.00 Mg 1.0 2.0 1050 11.2 1200 50 145 -12 〇 42 1.010 Dy3.0 Mn 1.20 Mg 1.0 2.0 1050 10.5 1000 - - - - 43 1.010 Dy3.0 V0.50 Mg 1.0 2.0 1050 11.3 1200 50 145 -12 〇 44 1.010 Dy3.0 Mn0.50 Mg 0.2 2.0 1050 9.6 800 - - - - 45 1.010 Dy3.0 Mn 0.50 Mg 0.3 2.0 1050 11.0 1200 22 145 -12 〇 46 1.010 Dy3.0 Mn0.50 Mg 3.0 2.0 1050 11.2 1100 23 145 12 〇 47 1.010 Dy3.0 Mn 0.50 Mg 4.0 2.0 1050 11.0 1000 25 145 •12 〇 48 1.010 Dy3.0 Mn 0.50 Mg 5.0 2.0 1050 10.4 700 - - - - 49 1.010 Dy3.0 Mn 0.50 Ni 2.0 2.0 1050 11.1 1150 22 145 -12 〇 50 1.010 Dy 3.0 Mn 0.50 Zn 2.0 2.0 1050 11.2 1150 23 145 -12 〇 51 1.010 Dy3.0 Mn 0.50 Mg 1.0 0.1 1200 - - - - - - 52 1.010 Dy3,0 Mn 0.50 Mg 1.0 0.2 1150 12.3 1000 20 145 -12 〇 53 1.010 Dy3.0 Mn 0.50 Mg 1.0 1.0 1050 12.1 1100 40 145 -12 〇 54 1.010 Dy3.0 Mn 0.50 Mg 1.0 5.0 1050 11.3 1300 30 145 -12 〇 55 1.010 Dy3.0 Mn 0.50 Mg 1.0 6.0 1050 9.8 800 - - - - 56 1.010 Y3.0 Mn 0.50 Mg 1.0 2.0 1050 12.1 1300 30 145 -12 〇 57 1.010 La 3.0 Mn0.50 Mg 1.0 2.0 1050 11.8 1200 30 143 -15 〇 58 1.010 Ce3.0 Mn 0.50 Mg 1,0 2.0 1050 11.8 1300 35 143 -15 〇 59 1.010 Pr3.0 Mn 0.50 Mg 1.0 2.0 1050 11.9 1200 35 143 -15 〇 60 1.010 Nd3.0 Mn 0.50 Mg 1.0 2.0 1050 12.1 1200 35 144 -13 〇 61 1.010 Sm 3.0 Mn 0.50 Mg 1.0 2.0 1050 12.1 1100 40 145 -12 〇 62 1.010 Eu3.0 Mn 0.50 Mg 1.0 2.0 1050 12.2 1300 40 145 -12 〇 63 1.010 Tb3.0 Mn 0.50 Mg 1.0 2.0 1050 12.3 1300 40 145 -12 〇 64 1.010 Ho 3.0 Mn0.50 Mg 1.0 2.0 1050 12.1 1400 40 146 -12 0 65 1.010 Er3.0 Mn 0.50 Mg 1.0 2.0 1050 12.1 1300 30 146 -12 〇 66 1.010 Tm3.0 Mn 0.50 Mg 1.0 2.0 1050 11.8 1200 30 146 -12 .〇 126515.doc -22- 1356048 67 1.010 Yb3.0 Mn0.50 Mg 1.0 2.0 1050 11.8 1200 25 146 -12 〇 68 1.010 Lu3.0 Mn0.50 Mg 1.0 2.0 1050 11.8 1200 25 145 •12 〇 69 1.010 Dy4.2 Erl.8 Mn0.50 Mg 1.0 2.0 1050 12.2 1000 50 145 -12 〇 70 1.010 Dy3.6 Yb2.4 Mn 0.50 Mg 1.0 2.0 1050 12.3 1000 50 144 -12 〇 71 1.010 Y3.6 Lu 2.4 Mn 0.50 Mg 1.0 2.0 1050 12.2 1000 50 143 •12 〇 試料編號31及35之試料之主成分m值在本發明之範圍 外,對於以Ni為内部電極之薄層之積層陶瓷電容,不能得 到足夠之絕緣電阻及信賴性。
試料編號 32〜34、37〜41、43、45~47、49、50、52~54、 56〜71之試料,對於以Ni為内部電極之薄層之積層陶瓷電 容,也能得到足夠之絕緣電阻及信賴性、且對X9R特性或 ει·也無不良影響。 又,試料編號36及42之試料,選自Mn及v中之至少1種 之含有量在本發明之較佳範圍外;試料編號料及48之試 料’選自Mg、Ni、Zn中之至少!種之含有量在本發明之較 佳範圍外;試料編號51及55之試料,以之含有量在本發明 <平又1芏摩&固夕卜
,,”v , ^ W电你 < 碍臂I 積層陶Η容,不能取得足夠之絕緣電阻及信賴性。作 是热對於單板電容或無需還原環氣氛培之積層電容,則可 足夠使用。 之試料為本發明範圍外 又,實驗例1〜3之表丨〜3中附有* 之試料。 【圖式簡單說明】 明之—實施形態之積層 圖1係以圖解方式表示基於本發 陶瓷電容1之剖面圖。 126515.doc •23. 1356048 【主要元件符號說明】 1 積層陶瓷電容 2 陶瓷積層體 3 介電質陶瓷層 4、5 内部電極 8 ' 9 外部電極 10、11 第1電鍍層 12、13 第2電鍍層 126515.doc -24-
Claims (1)
1356048 I公告本I 十、申請專利範圍·· 第096145761號專利申請案 中文申請專利範圍替換本(100年ί〇月)] 上y ίΐ i·—種介電質陶瓷,其係將以組成式· : (Bai x yCaxSnj^JTibzZrdO3表示之鈣鈦礦型化合物(其中前述 x、y、z、m分別滿足 0 990 SmSl.015、OSxg 0.20、 yg 〇·2〇、og 〇 〇5)作為主成分,對於前述主成 分100莫耳份包f 0.5〜20莫耳份RE(其中RE係選自Υ、 La、Ce、pr、Nd、Sm、Eu、Gd、Tb、Dy、Ho、Er、 Tm、Yb及Lu中之至少一種)作為副成分。 _ 2.如晴求項1之介電質陶瓷,其中在前述主成分中,前述x 為 0.02 $ X$ 〇.2〇。 .如叫求項1或2之介電質陶瓷,其中居裏溫度為13〇。〇以 上。 4·如請求項1或2之介電質陶瓷,其中,對於前述主成分 100莫耳份包含〇 〇2〜i莫耳份選自及V中之至少1種作 為副成分β # 5.如請求項1或2之介電質陶竞,其中,對於前述主成分 100莫耳份包含0 3〜4莫耳份選自Mg、Ni、Ζη中之至少1 種作為副成分。 6. 如請求項!或2之介電質陶竞,其中,對於前記主成分 100莫耳份包含G2〜5莫耳份Si作為副成分。 7. -種積層陶瓷電容’其係對於包括複數個積層之陶瓷層 及沿其界面形成之複數個層狀内部電極之陶兗積層體, 為了電氣連接露出於前記陶究積層體之表面之内部電極 而形成有複數個外部電極;其特徵在於: 126515-1001 〇31 .doc 1356048 前述陶瓷層包含如請求項1〜6中任一項之介電質陶 瓷。 8.如請求項7之積層陶瓷電容,其中前述内部電極之主成 分為Ni。 126515-1001031.doc
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